Silicon-supported ionic liquid catalyst

An ionic liquid, imidazole ionic liquid technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of insufficient catalyst efficiency and selectivity, short cycle life and other problems, to achieve the effects of easy control, increased cycle times, and high conversion rate

Active Publication Date: 2016-06-08
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical solution of the present invention is to provide a supported silicon-type ionic liquid catalyst for synthesizing ethylene carbonate in order to overcome the disadvantages of catalyst efficiency and selectivity that are not high enough in the prior art, use of auxiliary catalysts or solvents, and short cycle life.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Mix 24mL of N-methylimidazole and 20mL of 2-chloroethanol into a round-bottomed flask with a reflux condenser, under nitrogen protection, stir in a water bath at 80°C for 24h, stop the reaction, and dilute the obtained light yellow liquid with diethyl ether repeatedly Extracted 4 times, placed in a vacuum drying oven at 80°C, -0.09MPa and distilled under reduced pressure for 12h to obtain 1-(2-hydroxyethyl)-3-methylchloroimidazolium ionic liquid [HeMIM]Cl with a yield of 94 %.

[0051] Add 12mL tetraethyl orthosilicate (TEOS) and 8mL ethanol into a 100mL round-bottomed flask, place in a heating magnetic stirrer, mix and heat to 60°C. When the mixed system became clear, the ionic liquid [HeMIM]Cl was added (the molar ratio of [HeMIM]Cl to TEOS was 2:1). Under the action of stirring, it gradually becomes an oil bead suspension system. After continuing to react for 5 hours, start to add 24mL of hydrochloric acid dropwise. The color of the system gradually becomes lighter,...

Embodiment 2

[0054] Put 9.63mL of N-methylimidazole in a 100ml three-neck flask, add 9.5g of chloroacetic acid in three batches, and after the chloroacetic acid is completely dissolved, place the reaction in a water bath at 70°C for 10 hours to obtain a light yellow liquid. Pour it into a beaker and wash it repeatedly with ether for 3 times, put it in a vacuum drying oven at 80°C, -0.09MPa and distill for 12 hours under reduced pressure to obtain 1-carboxyethyl-3-methylimidazolium chloride ionic liquid [CeMIM]Cl, Yield 91%.

[0055] Add 12mL tetraethyl orthosilicate (TEOS) and 8mL ethanol into a 100mL round-bottomed flask, place in a heating magnetic stirrer, mix and heat to 60°C. When the mixed system became clear, the ionic liquid [CeMIM]Cl was added (the molar ratio of [CeMIM]Cl to TEOS was 2:1), and the oily bead-like liquid began to form, and white foam appeared after 1.5 hours, and a small part of it solidified after 100 minutes. After 4 hours of reaction, 24mL of HCl was added drop...

Embodiment 3

[0058] In the same equipment used in Example 2, under the same conditions, just change the amount of ionic liquid added, the amount of [CeMIM]Cl and TEOS and the molar ratio is 3:1, the catalyst is supported silicon type chloride 1-carboxylate Ethyl-3-methylimidazolium ionic liquid [CeMIM]Cl-Si, its catalyzed reaction nearly 40min observes that the carbon dioxide mass flow count value does not change, after the completion of the reaction, the purity of the ethylene carbonate product is 98.4%, and the calculated epoxy The conversion of ethane was 98.1%, and the yield of ethylene carbonate was 96.5%.

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Abstract

The present invention belongs to the technical field of catalysts, and relates to a silicon-supported ionic liquid catalyst. First methylimidazole or alkyl imidazole is reacted with a halogen-substituted alkyl alcohol / acid to prepare an imidazole ionic liquid with reactive groups for standby use; then tetraethylorthosilicate and ethanol are added into a fixed volume container for mixing and heating, then stirred, and then added dropwise into a mixed ionic liquid solution, hydrochloric acid is added dropwise while stirring into a suspension system, and the suspension system is gradually solidified into a gel; and finally at 60 DEG C the gel is aged for 2-6h, the gel-like system is dried to give a solid product, and the solid product is ground into pale yellow powder, namely the silicon-supported ionic liquid catalyst Advantages of the silicon-supported ionic liquid catalyst are as follows: the silicon-supported ionic liquid catalyst has good catalytic synergy effect and base position isolation effect, high activity and selectivity, and can be recycled. Auxiliary catalysts or solvents are not used in catalytic processes, and high yield and high purity ethylene carbonate new products can be obtained under relatively mild conditions.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a silicon-supported ionic liquid catalyst, in particular to a catalyst for preparing ethylene carbonate by catalyzing the cycloaddition reaction of carbon dioxide and ethylene oxide. Background technique [0002] Ethylene carbonate is a good solvent for the production of polyamide, polyacrylonitrile, polyvinyl chloride and other high polymers. It can also be used as spinning liquid and other chemical auxiliary agents in textiles. It can also be used as a solvent for removing industrial acid gases and Additives for concrete. In medicine, it can be used as a pharmaceutical component and an organic synthesis intermediate, and can also be used as a plastic foaming agent and a stabilizer for synthetic lubricating oil. In the capacitor battery industry, the mixed solution of EC and propylene carbonate has a high dielectric constant and can be used as an electrolyte for lithium batteri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07D317/38
Inventor 郭立颖史君贺俊海程光剑黄集钺吕洁李志宇田振英曹微王红韩秋萍
Owner PETROCHINA CO LTD
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